WO2013089185A1 - Film réfléchissant les infrarouges - Google Patents
Film réfléchissant les infrarouges Download PDFInfo
- Publication number
- WO2013089185A1 WO2013089185A1 PCT/JP2012/082347 JP2012082347W WO2013089185A1 WO 2013089185 A1 WO2013089185 A1 WO 2013089185A1 JP 2012082347 W JP2012082347 W JP 2012082347W WO 2013089185 A1 WO2013089185 A1 WO 2013089185A1
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- WIPO (PCT)
- Prior art keywords
- protective layer
- layer
- infrared
- reflective film
- infrared reflective
- Prior art date
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- 239000011241 protective layer Substances 0.000 claims abstract description 68
- 239000010410 layer Substances 0.000 claims abstract description 64
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 48
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229920000642 polymer Polymers 0.000 claims abstract description 41
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 238000010894 electron beam technology Methods 0.000 claims description 32
- 239000000126 substance Substances 0.000 claims description 17
- 230000001678 irradiating effect Effects 0.000 claims description 5
- 239000002904 solvent Substances 0.000 abstract description 43
- 229920002239 polyacrylonitrile Polymers 0.000 abstract description 11
- 229920003214 poly(methacrylonitrile) Polymers 0.000 abstract description 4
- 238000007922 dissolution test Methods 0.000 abstract 4
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 24
- 239000000463 material Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- 238000007740 vapor deposition Methods 0.000 description 11
- 229920000459 Nitrile rubber Polymers 0.000 description 10
- 229910044991 metal oxide Inorganic materials 0.000 description 10
- 150000004706 metal oxides Chemical class 0.000 description 10
- 125000004432 carbon atom Chemical group C* 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 8
- 125000004093 cyano group Chemical group *C#N 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 239000000178 monomer Substances 0.000 description 8
- -1 polyethylene terephthalate Polymers 0.000 description 8
- 239000005357 flat glass Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 description 6
- 239000005020 polyethylene terephthalate Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 239000012790 adhesive layer Substances 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 229910002668 Pd-Cu Inorganic materials 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- JAONJTDQXUSBGG-UHFFFAOYSA-N dialuminum;dizinc;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Zn+2].[Zn+2] JAONJTDQXUSBGG-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 238000007733 ion plating Methods 0.000 description 2
- 238000001755 magnetron sputter deposition Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- MFJDFPRQTMQVHI-UHFFFAOYSA-N 3,5-dioxabicyclo[5.2.2]undeca-1(9),7,10-triene-2,6-dione Chemical compound O=C1OCOC(=O)C2=CC=C1C=C2 MFJDFPRQTMQVHI-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- 229910002695 AgAu Inorganic materials 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910017073 AlLi Inorganic materials 0.000 description 1
- 241001136782 Alca Species 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- DEZRYPDIMOWBDS-UHFFFAOYSA-N dcm dichloromethane Chemical compound ClCCl.ClCCl DEZRYPDIMOWBDS-UHFFFAOYSA-N 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- BDVZHDCXCXJPSO-UHFFFAOYSA-N indium(3+) oxygen(2-) titanium(4+) Chemical compound [O-2].[Ti+4].[In+3] BDVZHDCXCXJPSO-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- AHLBNYSZXLDEJQ-FWEHEUNISA-N orlistat Chemical compound CCCCCCCCCCC[C@H](OC(=O)[C@H](CC(C)C)NC=O)C[C@@H]1OC(=O)[C@H]1CCCCCC AHLBNYSZXLDEJQ-FWEHEUNISA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- YVTHLONGBIQYBO-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) Chemical compound [O--].[Zn++].[In+3] YVTHLONGBIQYBO-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/28—Interference filters
- G02B5/281—Interference filters designed for the infrared light
- G02B5/282—Interference filters designed for the infrared light reflecting for infrared and transparent for visible light, e.g. heat reflectors, laser protection
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
-
- G02B1/105—
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/208—Filters for use with infrared or ultraviolet radiation, e.g. for separating visible light from infrared and/or ultraviolet radiation
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
- G02B5/26—Reflecting filters
Definitions
- the present invention relates to an infrared reflective film having high transparency in the visible light region and high reflectivity in the infrared light region.
- the infrared reflective film is mainly used for suppressing the thermal effect of the emitted sunlight.
- an infrared reflecting film is pasted on a window glass of a building or an automobile, so that infrared rays (particularly near infrared rays) that enter the room through the window glass are shielded and the temperature rise in the room is thereby suppressed. It is possible to save energy by suppressing power consumption.
- Patent Document 1 discloses using polyacrylonitrile (PAN) as a material for the protective layer.
- PAN polyacrylonitrile
- Polymers such as polyacrylonitrile have a low infrared absorptivity and can shield far-infrared rays emitted from the room through the translucent member. Energy saving can also be achieved by the heat insulation effect.
- the protective layer is prepared by first dissolving the polymer in a solvent to prepare a solution, and then applying this solution on the infrared reflective layer. Is dried (the solvent is volatilized).
- this kind of infrared reflective film is stuck on a window glass of a building or an automobile so that the protective layer is on the front side. Therefore, dirt or the like adheres to the surface of the protective layer as time passes.
- the surface of the protective layer may be cleaned using, for example, a cleaning liquid.
- the cleaning liquid often contains various organic solvents. And, when at least a part of the organic solvent contained in the cleaning liquid is a solvent soluble in the polymer contained in the protective layer, the protective layer is eluted during cleaning, and the infrared reflective layer having low scratch resistance is exposed. The problem arises.
- the present invention has been made in view of such circumstances, and an object thereof is to provide an infrared reflective film excellent in solvent resistance.
- Infrared reflective film An infrared reflective film in which a reflective layer and a protective layer are sequentially laminated on one surface of a substrate,
- the protective layer is a layer containing a polymer containing a repeating unit A of the following chemical formula I,
- the gel fraction after each solubility test of the solubility test for methyl ethyl ketone, the solubility test for dimethylformamide, and the solubility test for methylene chloride is 65% or more.
- an infrared reflective film in which a reflective layer and a protective layer are sequentially laminated on one surface of a substrate,
- the protective layer is a layer containing a polymer containing at least any two or more repeating units among the repeating units A, B and C of the following chemical formula II,
- the gel fraction after each solubility test of the solubility test for methyl ethyl ketone, the solubility test for dimethylformamide, and the solubility test for methylene chloride is 65% or more.
- the protective layer may have a crosslinked structure of the polymer.
- the crosslinked structure can be formed by irradiating the protective layer with an electron beam.
- the vertical emissivity of the surface on the protective layer side can be 0.20 or less.
- an infrared reflective film excellent in solvent resistance can be provided.
- the infrared reflective film which concerns on this embodiment is an infrared reflective film which has a heat insulation characteristic (reflective characteristic of far infrared rays) in addition to the thermal insulation characteristic (reflective characteristic of near infrared rays) which the conventional infrared reflective film has.
- a reflective layer 2 and a protective layer 3 are laminated in that order on one surface 1a of a substrate 1, and an adhesive layer 4 is provided on the other surface 1b. It has a layer structure.
- a polyester film is used as the substrate 1.
- a film made of polyethylene terephthalate, polyethylene naphthalate, polypropylene terephthalate, polybutylene terephthalate, polycyclohexylene methylene terephthalate, or a mixed resin in which two or more of these are combined is used.
- a polyethylene terephthalate (PET) film is preferable from the viewpoint of performance, and a biaxially stretched polyethylene terephthalate (PET) film is particularly preferable.
- the reflective layer 2 is a vapor deposition layer formed by vapor deposition on the surface (one surface) 1a of the substrate 1.
- Examples of the method for forming the vapor deposition layer include physical vapor deposition (PVD) such as sputtering, vacuum vapor deposition, and ion plating.
- PVD physical vapor deposition
- the reflective layer 2 is formed on the substrate 1 by heating and evaporating the vapor deposition material by a method such as resistance heating, electron beam heating, laser beam heating, or arc discharge in vacuum.
- a vacuum containing an inert gas such as argon cations such as Ar + accelerated by glow discharge are bombarded on the target (vapor deposition material) to vaporize the vapor deposition material.
- the reflective layer 2 is formed on the substrate 1.
- Ion plating is a vapor deposition method that combines vacuum vapor deposition and sputtering. In this method, the evaporation layer released by heating is ionized and accelerated in an electric field in vacuum, and is deposited on the substrate 1 in a high energy state, whereby the reflective layer 2 is formed.
- the reflective layer 2 has a multi-layer structure in which a translucent metal layer 2a is sandwiched between a pair of metal oxide layers 2b and 2c. Surface) 1a, a metal oxide layer 2b is deposited, then a semitransparent metal layer 2a is deposited on the metal oxide layer 2b, and finally a metal oxide layer 2c is deposited on the semitransparent metal layer 2a. Formed.
- the translucent metal layer 2a includes, for example, aluminum (Al), silver (Ag), silver alloy (MgAg, Ag—Pd—Cu alloy (APC), AgCu, AgAuCu, AgPd, AgAu, etc.), aluminum alloy (AlLi, AlCa) , AlMg, etc.), or a metal material in which two or more of these are combined.
- the metal oxide layers 2b and 2c are for imparting transparency to the reflective layer 2 and preventing deterioration of the translucent metal layer 2a.
- ITO indium tin oxide
- IT indium titanium oxide
- An oxide such as indium zinc oxide (IZO), gallium zinc oxide (GZO), aluminum zinc oxide (AZO), or indium gallium oxide (IGO) is used.
- the protective layer 3 is a layer containing a polymer containing the repeating unit A of the following chemical formula I.
- R1 in Chemical Formula I H or a methyl group can be used.
- R1 is polyacrylonitrile (PAN).
- PAN polyacrylonitrile
- PMAN polymethacrylonitrile
- the protective layer 3 is prepared by dissolving the above-described polymer in a solvent (with a crosslinking agent if necessary), applying the solution on the reflective layer 2, and then drying the solution (solvent Is volatilized).
- the solvent is a solvent in which the above-described polymer is soluble, and for example, a solvent such as methyl ethyl ketone (MEK) is used.
- the ratio of the repeating unit of the chemical formula I contained in the polymer to the whole polymer is 10% by weight or more as a lower limit. Preferably, it is 20% by weight or more. More preferably, it is 30% by weight or more. Moreover, as an upper limit, it is 100 weight% or less. Preferably, it is 80 weight% or less. More preferably, it is 65% by weight or less. If it is the said range, a favorable heat insulation characteristic can be provided to an infrared reflective film.
- the lower limit of the thickness of the protective layer 3 is 1 ⁇ m or more. Preferably, it is 3 ⁇ m or more. Moreover, as an upper limit, it is 20 micrometers or less. Preferably, it is 15 ⁇ m or less. More preferably, it is 10 ⁇ m or less.
- the thickness of the protective layer 3 is small, the infrared reflection characteristics are enhanced, but the scratch resistance is impaired, and the function as the protective layer 3 cannot be sufficiently exhibited. If the thickness of the protective layer 3 is large, the heat insulating property of the infrared reflective film is deteriorated. When the thickness of the protective layer 3 is within the above range, the protective layer 3 that can absorb the infrared rays and can appropriately protect the reflective layer 2 is obtained.
- the spectral reflectance ⁇ n is measured in the wavelength range of 5 to 50 ⁇ m of room temperature thermal radiation.
- the wavelength region of 5 to 50 ⁇ m is the far infrared region, and the vertical emissivity decreases as the reflectance in the far infrared wavelength region increases.
- the protective layer 3 is a layer containing a polymer containing at least any two or more repeating units among the repeating unit A of the following chemical formula II (same as the repeating unit A of the chemical formula I), B and C.
- R1 in Chemical Formula II H or a methyl group can be used.
- R2 to R5 in Chemical Formula II H and an alkyl group or alkenyl group having 1 to 4 carbon atoms can be used.
- hydrogenated nitrile rubber (HNBR) is composed of repeating units A, B and C, and H is used as R1 to R5.
- acrylonitrile (repeating unit D) and derivatives thereof as shown in Chemical Formula III
- alkyl having 4 carbon atoms (repeating unit E) and derivatives thereof
- butadiene And a copolymer of the repeating unit F1 or F2) and derivatives thereof.
- R6 represents H or a methyl group
- R7 to R18 represent H or an alkyl group having 1 to 4 carbon atoms.
- F1 and F2 represents a repeating unit in which butadiene is polymerized, and F1 is a main repeating unit.
- nitrile rubber or nitrile rubber which is a copolymer of acrylonitrile (repeating unit D) and its derivatives of formula III, 1,3-butadiene (repeating unit F1) and its derivatives.
- Hydrogenated nitrile rubber in which part or all of the double bond is hydrogenated may be used.
- the butadiene on the left side is bonded to the side to which the cyano group (—CN) of acrylonitrile is bonded, and the butadiene on the right side is formed to the side to which the cyano group (—CN) of acrylonitrile is not bonded.
- one repeating unit A, one repeating unit B, and two repeating units C are included.
- the repeating unit A includes a carbon atom in which the carbon atom on the right side of the butadiene on the left side is bonded to the cyano group (—CN) of acrylonitrile, and the repeating unit B is bonded to the cyano group (—CN) of acrylonitrile.
- the leftmost carbon atom of the left butadiene and the rightmost carbon atom of the right butadiene become part of the repeating unit A or the repeating unit B depending on the type of molecule to be bonded.
- the protective layer 3 is prepared by dissolving the above-described polymer in a solvent (with a crosslinking agent if necessary), applying the solution on the reflective layer 2, and then drying the solution (solvent Is volatilized).
- the solvent is a solvent that can dissolve the above-described polymer, and for example, a solvent such as methyl ethyl ketone, dimethylformamide (DMF), or methylene chloride (dichloromethane) is used.
- Methyl ethyl ketone and methylene chloride are low boiling point solvents (methyl ethyl ketone is 79.5 ° C., methylene chloride is 40 ° C.).
- the solvent can be volatilized at a low drying temperature, so that the substrate 1 (or the reflective layer 2) is not damaged by heat.
- dimethylformamide has a boiling point of 153 ° C., if it is dried at a temperature lower than this, the substrate 1 (or the reflective layer 2) will not be damaged by heat.
- methyl ethyl ketone and methylene chloride are preferable to dimethylformamide in that the drying time can be greatly reduced.
- the protective layer 3 preferably has a cross-linked structure between polymers.
- the solvent resistance of the protective layer 3 is improved, so that the protective layer 3 is prevented from eluting even when a solvent soluble in the polymer contacts the protective layer 3. can do.
- the cumulative irradiation dose of the electron beam is 50 kGy or more as a lower limit value. Preferably, it is 100 kGy or more. More preferably, it is 200 kGy or more. Moreover, as an upper limit, it is 1000 kGy or less. Preferably, it is 600 kGy or less. More preferably, it is 400 kGy or less.
- the cumulative irradiation dose refers to the irradiation dose when the electron beam is irradiated once, and the total irradiation dose when the electron beam is irradiated a plurality of times.
- the single irradiation dose of the electron beam is preferably 300 kGy or less. If the integrated irradiation dose of the electron beam is within the above range, sufficient crosslinking between the polymers can be obtained. Moreover, if the integrated irradiation dose of the electron beam is within the above range, yellowing of the polymer and the substrate 1 generated by the electron beam irradiation can be minimized, and an infrared reflective film with less coloring can be obtained. Can do.
- These electron beam irradiation conditions are irradiation conditions at an acceleration voltage of 150 kV.
- a crosslinking agent such as a polyfunctional monomer such as a radical polymerization type monomer when the polymer is dissolved in the solvent or after the polymer is dissolved in the solvent.
- a polyfunctional monomer such as a radical polymerization type monomer
- radical polymerization monomers of (meth) acrylate monomers are preferred.
- the accumulated irradiation dose of the electron beam can be completed with a low irradiation dose. Moreover, yellowing of the polymer and the substrate 1 can be further suppressed by reducing the cumulative irradiation dose of the electron beam, and productivity can be improved.
- the amount of the additive added increases, the vertical emissivity of the surface of the infrared reflecting film on the protective layer 3 side (based on the reflective layer 2) deteriorates.
- the amount of the additive added is preferably 1 to 35% by weight with respect to the polymer. More preferably, it is 2 to 25% by weight based on the polymer.
- the thickness of the layer structure on the reflective layer 2, that is, the thickness of the protective layer 3 is reduced to protect (based on the reflective layer 2).
- the vertical emissivity of the surface on the layer 3 side is small.
- the protective layer 3 is made of nitrile rubber, hydrogenated nitrile rubber, fully hydrogenated nitrile rubber, or the like, which hardly absorbs far-infrared rays and is easily transmitted, the vertical emissivity is also reduced. Accordingly, far infrared rays are not easily absorbed by the protective layer 3 even if they are incident on the protective layer 3, reach the reflective layer 2, and as a result, are easily reflected by the reflective layer 2.
- the infrared reflective film according to the present embodiment by sticking the infrared reflective film according to the present embodiment to a light transmissive member such as a window glass from the indoor side, it is possible to shield far infrared rays emitted from the room through the light transmissive member to the outside. In this way, a heat insulation effect can be expected in winter and at night when the indoor temperature decreases.
- the vertical emissivity of the surface on the protective layer 3 side is set to 0.20 or less for the purpose. More preferably, the vertical emissivity is 0.15 or less.
- the translucency of a translucent member is not inhibited by making visible light transmittance (refer JIS A5759) high.
- the visible light transmittance is set to 50% or more for the purpose.
- the infrared reflective film according to the present embodiment to a light transmissive member such as a window glass from the indoor side, the near infrared light incident on the room through the light transmissive member such as the window glass is shielded.
- a heat shielding effect in summer can be expected.
- the solar radiation transmittance (see JIS A5759) when light is incident from the surface of the substrate 1 (based on the reflective layer 2) is 60% or less.
- the favorable solvent resistance is provided to the protective layer 3 as mentioned above. That is, the solvent resistance of the protective layer 3 is improved by crosslinking the polymers in the protective layer 3 together. Accordingly, even when a solvent capable of dissolving a polymer comes into contact with the protective layer 3, it is possible to prevent the protective layer 3 from being eluted. Can be prevented from decreasing.
- the gel fraction after each solubility test in a solubility test for methyl ethyl ketone, a solubility test for dimethylformamide, and a solubility test for methylene chloride is 65% or more. Is set. However, it is preferably 70% or more. More preferably, it is 80% or more. Even more preferably, it is 90% or more. These are clarified by test results of various examples described later.
- the present inventors produced an infrared reflective film according to the present embodiment (Example), together with an infrared reflective film for comparison (Comparative Example), and a solvent resistance test for them. Went. The inventors also measured their vertical emissivity.
- the manufacturing method is as follows in both the examples and comparative examples.
- a polyethylene terephthalate film (trade name “Diafoil T602E50” manufactured by Mitsubishi Plastics, Inc.) having a thickness of 50 ⁇ m was used as the substrate 1.
- a reflective layer 2 was formed on one surface 1a of the substrate 1 by DC magnetron sputtering. Specifically, using a DC magnetron sputtering method, a metal oxide layer 2b made of indium tin oxide is formed with a thickness of 35 nm on one surface 1a of the substrate 1, and a translucent made of an Ag—Pd—Cu alloy is formed thereon.
- the metal layer 2a was formed with a thickness of 18 nm, and the metal oxide layer 2c made of indium tin oxide was formed thereon with a thickness of 35 nm.
- a protective layer 3 was formed on the reflective layer 2 by a coating method. In addition, the detailed formation conditions of the protective layer 3 are explained in full detail in description of an Example and a comparative example, respectively.
- the measurement method of vertical emissivity is as follows. Using a Fourier transform infrared spectroscopic (FT-IR) device (Varian) equipped with a variable angle reflection accessory, the regular reflectance of infrared light having a wavelength of 5 to 25 microns was measured, and JIS R 3106- It calculated
- FT-IR Fourier transform infrared spectroscopic
- Example 1 10% by weight of polyacrylonitrile (manufactured by Aldrich) [k: 100, 1: 0, m: 0, R1: H] and 90% by weight of dimethylformamide (manufactured by Wako Pure Chemical Industries, Ltd.) are mixed and dissolved with stirring. The reaction was carried out at a temperature of 5 ° C. for 5 hours, and polyacrylonitrile was dissolved in a dimethylformamide solvent to prepare a solution. And the solution was apply
- an electron beam was irradiated from the surface side of the protective layer 3 using an electron beam irradiation apparatus (product name “EC250 / 30/20 mA” manufactured by Iwasaki Electric Co., Ltd.), and an infrared reflective film according to Example 1 was obtained.
- the electron beam irradiation conditions were a line speed of 3 m / min, an acceleration voltage of 150 kV, and an integrated irradiation dose of 600 kGy.
- an electron beam having a single irradiation dose of 200 kGy was irradiated three times.
- Example 2 As a material used for the protective layer, instead of polyacrylonitrile, hydrogenated nitrile rubber (trade name “Terban 3407” manufactured by LANXESS) [k: 20.5, l: 79.5, m: 0, R1 to R3: H] Example 1 except that a solvent of methyl ethyl ketone (manufactured by Wako Pure Chemical Industries, Ltd.) was used instead of the solvent of dimethylformamide, and the drying time was 120 ° C. instead of 150 ° C. Is the same.
- hydrogenated nitrile rubber (trade name “Terban 3407” manufactured by LANXESS) [k: 20.5, l: 79.5, m: 0, R1 to R3: H]
- Example 1 except that a solvent of methyl ethyl ketone (manufactured by Wako Pure Chemical Industries, Ltd.) was used instead of the solvent of dimethylformamide, and the drying time was 120 ° C. instead of 150 ° C. I
- Example 3 Hydrogenated nitrile rubber (trade name “Terban 4367” manufactured by LANXESS [k: 27.4, l: 69.1, m: 3.5, R1 to R5: H]) was used as a material for the protective layer. Except for this point, the second embodiment is the same as the second embodiment.
- Example 4 Other than the use of hydrogenated nitrile rubber (trade name “Telvan 5065” [k: 33.3, l: 63, m: 3.7, R1 to R5: H] manufactured by LANXESS) as the material used for the protective layer Is the same as in Example 2.
- hydrogenated nitrile rubber trade name “Telvan 5065” [k: 33.3, l: 63, m: 3.7, R1 to R5: H] manufactured by LANXESS
- Example 4 is the same as Example 4 except that the electron beam irradiation dose is set to 100 kGy.
- Example 4 is the same as Example 4 except that the electron beam irradiation dose is set to 1000 kGy. In this example, an electron beam having a single irradiation dose of 200 kGy was irradiated five times.
- Example 1 is the same as Example 1 except that no electron beam is irradiated.
- Example 2 is the same as Example 2 except that the electron beam is not irradiated.
- Example 4 is the same as Example 4 except that the electron beam irradiation dose is 50 kGy.
- Example 4 It is the same as Example 4 except the point which irradiated with the ultraviolet-ray instead of irradiating an electron beam. More specifically, after forming the protective layer 3 having a thickness of 5 ⁇ m, ultraviolet rays are irradiated from the surface side of the protective layer 3 using an ultraviolet irradiation device (product name “UE021-203C” manufactured by Eye Graphics Co., Ltd.). The infrared reflective film which concerns on the comparative example 4 was obtained. The irradiation dose of ultraviolet rays was 1000 mJ / cm 2 .
- the infrared reflective film which concerns on this invention is not limited to the said embodiment, A various change is possible in the range which does not deviate from the summary of this invention.
- the polymer composed of only the repeating unit A or at least any two or more repeating units among the repeating units A, B, and C has been described.
- the present invention is not limited to this.
- Other repeating units other than these repeating units can also be included as long as the properties required for the protective layer are not impaired.
- Other repeating units include, for example, styrene, ⁇ -methylstyrene, (meth) acrylic acid, methyl (meth) acrylate, ethyl (meth) acrylate, 2-hydroxyethyl (meth) acrylate, vinyl acetate, (meth) acrylamide Etc.
- the ratio of these to the whole polymer is preferably 10% by weight or less.
- the reflective layer 2 is formed by vapor deposition.
- the present invention is not limited to this.
- a reflective layer may be prepared separately from the base material by using a reflective film, and the reflective layer may be formed by sticking the reflective film to the base material.
- the infrared reflective film according to the above embodiment is an infrared reflective film having both heat shielding properties and heat insulating properties.
- the present invention is not limited to this. Needless to say, the infrared reflective film according to the present invention can also be applied to an infrared reflective film having only a conventional heat shielding property.
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Abstract
La présente invention concerne un film réfléchissant les infrarouges, qui possède une couche réfléchissante et une couche protectrice déposées dans cet ordre sur une surface d'un substrat, et qui montre une excellente résistance aux solvants. La couche protectrice contient des polymères comprenant du polyacrylonitrile (PAN) et du polyméthacrylonitrile (PMAN), et présente un rapport de teneur en gel supérieur ou égal à 65 % après la réalisation de chacun des tests de dissolution suivants : un test de dissolution avec de la méthyléthylcétone, un test de dissolution avec du diméthylformamide et un test de dissolution avec du chlorure de méthylène.
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JP2011-276330 | 2011-12-16 | ||
JP2011276330 | 2011-12-16 | ||
JP2012132282A JP2013145358A (ja) | 2011-12-16 | 2012-06-11 | 赤外線反射フィルム |
JP2012-132282 | 2012-06-11 |
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WO2013089185A1 true WO2013089185A1 (fr) | 2013-06-20 |
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PCT/JP2012/082347 WO2013089185A1 (fr) | 2011-12-16 | 2012-12-13 | Film réfléchissant les infrarouges |
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Cited By (8)
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WO2016097599A1 (fr) | 2014-12-17 | 2016-06-23 | Saint-Gobain Glass France | Vitrage de controle thermique muni d'un film polymere protecteur |
FR3045034A1 (fr) * | 2015-12-15 | 2017-06-16 | Saint Gobain | Vitrage de controle thermique muni d'un film polymere protecteur |
WO2019106295A1 (fr) | 2017-11-30 | 2019-06-06 | Saint-Gobain Glass France | Vitrage fonctionnel muni d'un film protecteur permanent |
WO2019145361A1 (fr) | 2018-01-24 | 2019-08-01 | Noemille Participations | Procédé de traitement et d'assemblage de vitrage comprenant une couche á faible émissivité |
WO2020043973A1 (fr) | 2018-08-31 | 2020-03-05 | Saint-Gobain Glass France | Vitrage texture et isolant pour serre |
US10591653B2 (en) | 2016-02-05 | 2020-03-17 | Saint-Gobain Performance Plastics Corporation | Low corrosion solar control stack |
JP2022510109A (ja) * | 2018-11-14 | 2022-01-26 | サン-ゴバン グラス フランス | ガラス基材の層又は層の積層物の選択的エッチングのための方法 |
RU2774070C1 (ru) * | 2018-11-14 | 2022-06-15 | Сэн-Гобэн Гласс Франс | Способ селективного травления слоя или пакета слоев на стеклянной подложке |
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JPS57110443A (en) * | 1980-12-29 | 1982-07-09 | Teijin Ltd | Selective beam transmitting laminate |
JP2006047687A (ja) * | 2004-08-04 | 2006-02-16 | Dainippon Printing Co Ltd | 光学フィルタ及びプラズマディスプレイパネル |
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JPS57110443A (en) * | 1980-12-29 | 1982-07-09 | Teijin Ltd | Selective beam transmitting laminate |
JP2006047687A (ja) * | 2004-08-04 | 2006-02-16 | Dainippon Printing Co Ltd | 光学フィルタ及びプラズマディスプレイパネル |
Cited By (17)
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FR3030496A1 (fr) * | 2014-12-17 | 2016-06-24 | Saint Gobain | Vitrage de controle thermique muni d'un film polymere protecteur |
WO2016097599A1 (fr) | 2014-12-17 | 2016-06-23 | Saint-Gobain Glass France | Vitrage de controle thermique muni d'un film polymere protecteur |
FR3045034A1 (fr) * | 2015-12-15 | 2017-06-16 | Saint Gobain | Vitrage de controle thermique muni d'un film polymere protecteur |
WO2017103465A1 (fr) * | 2015-12-15 | 2017-06-22 | Saint-Gobain Glass France | Vitrage de controle thermique muni d'un film polymere protecteur |
CN108367974A (zh) * | 2015-12-15 | 2018-08-03 | 法国圣戈班玻璃厂 | 被提供有保护性聚合物膜的热控窗玻璃 |
US11098521B2 (en) | 2015-12-15 | 2021-08-24 | Saint-Gobain Glass France | Thermal control glazing with a protective polymer film |
RU2734354C2 (ru) * | 2015-12-15 | 2020-10-15 | Сэн-Гобэн Гласс Франс | Терморегулирующее остекление, снабженное защитной полимерной пленкой |
US10591653B2 (en) | 2016-02-05 | 2020-03-17 | Saint-Gobain Performance Plastics Corporation | Low corrosion solar control stack |
US11136263B2 (en) | 2017-11-30 | 2021-10-05 | Saint-Gobain Glass France | Functional glazing provided with a permanent protective film |
WO2019106295A1 (fr) | 2017-11-30 | 2019-06-06 | Saint-Gobain Glass France | Vitrage fonctionnel muni d'un film protecteur permanent |
RU2764848C2 (ru) * | 2017-11-30 | 2022-01-21 | Сэн-Гобэн Гласс Франс | Функциональное остекление, снабженное постоянной защитной пленкой |
WO2019145361A1 (fr) | 2018-01-24 | 2019-08-01 | Noemille Participations | Procédé de traitement et d'assemblage de vitrage comprenant une couche á faible émissivité |
FR3085372A1 (fr) | 2018-08-31 | 2020-03-06 | Saint-Gobain Glass France | Vitrage texture et isolant pour serre |
WO2020043973A1 (fr) | 2018-08-31 | 2020-03-05 | Saint-Gobain Glass France | Vitrage texture et isolant pour serre |
JP2022510109A (ja) * | 2018-11-14 | 2022-01-26 | サン-ゴバン グラス フランス | ガラス基材の層又は層の積層物の選択的エッチングのための方法 |
RU2774070C1 (ru) * | 2018-11-14 | 2022-06-15 | Сэн-Гобэн Гласс Франс | Способ селективного травления слоя или пакета слоев на стеклянной подложке |
JP7234358B2 (ja) | 2018-11-14 | 2023-03-07 | サン-ゴバン グラス フランス | ガラス基材の層又は層の積層物の選択的エッチングのための方法 |
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